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Water → HCID 178490339、化合物

HRID 2289717
ノート
印刷プレビュー

反応式

HRID 2289717 の反応式
[Cl:1]C1C2C(=CC(S(N(CC3C=CC=C(OC)C=3)CC(O)=O)(=O)=O)=CC=2)C([NH:29][C:30]([NH2:32])=[NH:31])=NC=1.[H-].[Na+].[C:35]([O:39][C:40](=[O:67])[CH2:41][N:42]([S:52]([C:55]1[CH:64]=[C:63]2[C:58]([C:59]([Cl:66])=[CH:60][N:61]=[C:62]2Cl)=[CH:57][CH:56]=1)(=[O:54])=[O:53])[CH2:43][C:44]1[CH:49]=[CH:48][CH:47]=[C:46]([O:50][CH3:51])[CH:45]=1)([CH3:38])([CH3:37])[CH3:36].O>COCCOC>[ClH:1].[C:35]([O:39][C:40](=[O:67])[CH2:41][N:42]([S:52]([C:55]1[CH:64]=[C:63]2[C:58]([C:59]([Cl:66])=[CH:60][N:61]=[C:62]2[NH:31][C:30]([NH2:32])=[NH:29])=[CH:57][CH:56]=1)(=[O:53])=[O:54])[CH2:43][C:44]1[CH:49]=[CH:48][CH:47]=[C:46]([O:50][CH3:51])[CH:45]=1)([CH3:36])([CH3:37])[CH3:38]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 18698239HCID 18698239、化合物HCID 178490340HCID 178490340、化合物

生成物 1

HCID 178490339HCID 178490339、化合物収率 53.8%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
60 °C

実験手順

N-[(4-Chloro-1-guanidino-7-isoquinolinyl)sulphonyl]-N-(3-methoxybenzyl)glycine ##STR22## Guanidine hydrochloride (149 mg, 1.55 mmol) was added in one portion to a suspension of NaH (35 mg, 80% dispersion by wt in mineral oil, 1.16 mmol) in DME (10 mL) and the mixture was heated at 60° C. under N2 for 30 min. N-[(1,4-Dichloro-7-isoquinolinyl)sulphonyl]-N-(3-methoxybenzyl)glycine t-butyl ester (200 mg, 0.39 mmol) was added and the mixture heated at 90° C. for 2 h. The cooled mixture was poured into water, extracted with EtOAc (×3), and the combined organic extracts were washed with brine, dried (Na2SO4) and evaporated in vacuo. The residue was dissolved in Et2O-EtOAc and a solution of HCl in Et2O (0.5 M) was added to give a precipitate. The solid was collected by filtration, triturated with EtOAc and then dried to give N-[(4-chloro-1-guanidino-7-isoquinolinyl)sulphonyl]-N-(3-methoxybenzyl)glycine t-butyl ester hydrochloride (124 mg, 0.21 mmol) as a white solid.

後処理

  1. temperaturethe mixture heated at 90° C. for 2 h
  2. extractionextracted with EtOAc (×3)
  3. washthe combined organic extracts were washed with brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated in vacuo
  6. dissolutionThe residue was dissolved in Et2O-EtOAc
  7. additiona solution of HCl in Et2O (0.5 M) was added
  8. customto give a precipitate
  9. filtrationThe solid was collected by filtration
  10. customtriturated with EtOAc
  11. customdried

出典と根拠

ORDレコード
ord-1302e4562f6e49d087473d1b2f1fab0f
出典データセット
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06093731

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート